CN109234834A - A kind of preparation method of super-hydrophobic acid fiber by polylactic - Google Patents
A kind of preparation method of super-hydrophobic acid fiber by polylactic Download PDFInfo
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- CN109234834A CN109234834A CN201811087899.XA CN201811087899A CN109234834A CN 109234834 A CN109234834 A CN 109234834A CN 201811087899 A CN201811087899 A CN 201811087899A CN 109234834 A CN109234834 A CN 109234834A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D11/00—Other features of manufacture
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The present invention relates to a kind of preparation methods of super-hydrophobic acid fiber by polylactic, it is characterized in that preparation has the substance octacosanol of low-surface-energy, then dissolve octacosanol and polylactic acid simultaneously and spinning solution is made in methylene chloride；Spinning solution, which enters, carries out electrostatic spinning on electrostatic spinning machine, obtain fiber；Super-hydrophobic acid fiber by polylactic is prepared using the techniques such as washing, oil and dry in fiber.The strength property of the acid fiber by polylactic of the main strength property and market purchasing of super-hydrophobic acid fiber by polylactic prepared by the present invention is close, illustrates that it is a kind of acid fiber by polylactic of qualification.Super-hydrophobic acid fiber by polylactic prepared by the present invention is spun into polylactic acid fiber fabrics, water droplet in its apparent contact angle range between 153 °~156 °, it is thus regarded that, acid fiber by polylactic prepared by the present invention has super-hydrophobicity.Whole simple production process of the present invention, cheap, production process environmental pollution is small, has a extensive future.
Description
Technical field
The invention belongs to super-hydrophobic textile technical fields, and in particular to a kind of preparation side of super-hydrophobic acid fiber by polylactic
Method.
Background technique
Superhydrophobic fabric refers to the fabric with the contact angle of water greater than 150 °.Superhydrophobic fabric has special superficiality
Can, it is widely used in the fields such as waterproof, antifouling and automatically cleaning, the research of superhydrophobic fabric has become the hot spot of research.It is super thin
Water finishing agent is usually a kind of low-surface energy substance, these low-surface energy substances are usually coated in fabric surface, thus, fabric
With ultra-hydrophobicity, common super-hydrophobic finishing agent has: fluoro-organosilane, dimethyl silicone polymer and long-chain fat silane
Deng.Currently, the preparation method of superhydrophobic fabric is more, such as: sol-gel method, vapour deposition process, plasma surface treatment method
With chemical etching method etc., these methods mainly arrange the surface of fiber.Chinese Patent Application No. 201010593300.7
Disclose the simple preparation method and purposes of superhydrophobic fibers, fabric, the patent be fibrous material is carried out it is isocyanate-modified,
Then low-surface energy substance is modified, isocyanates used in this method is not environmentally.Chinese Patent Application No.
201710513224.6 disclosing a kind of superhydrophobic fibers felt and preparation method thereof, this method is that fibrofelt is first placed into preparation
Primer resin solution in impregnate, Excess resin and solvent are squeezed after taking-up, is made by the techniques such as dry.This method be also
The surface of fiber is arranged, and is needed to use many solvents and resin etc., is caused serious pollution to the environment.It is whole after the surface of fiber carries out
Science and engineering skill is relatively complicated, the high requirements on the equipment.If fibrous material mixes low-surface energy substance during the preparation process, thus
Its own is with super-hydrophobicity, then fabric made of the fiber will also have the function of super-hydrophobic, such research is rarely reported.
Polylactic acid (PLA) fiber is one of 21 century " green fiber " most with prospects, is had stingless to skin
Swash, density is small, moisture transported permeable and it is comfortable and easy to wear the features such as；In addition, it is with the gloss, good drapability, smooth as silk
The advantages that property, degradable and no pollution to the environment.Polylactic resin can be prepared by direct polycondensation of lactic acid.Lactic acid can be by starch
Fermentation obtains, and starch source is extensive.The production method of acid fiber by polylactic has: dry spinning method, melt spinning method and electrostatic spinning
Method etc., wherein method of electrostatic spinning is to dissolve polylactic acid in a solvent in electrostatic field and under certain condition, and then solvent evaporates
And it is formed by curing the superfine fibre of nanoscale to submicron order, the method mixes with polylactic acid for other materials and provides possibility.
With the fast development of economic society, acid fiber by polylactic is applied to more and more fields, at this point, wanting to acid fiber by polylactic
Ask also higher and higher, if can be by polylactic acid imparting superhydrophobic, application will more extensively.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, a kind of preparation method of super-hydrophobic acid fiber by polylactic is provided.
The method comprises the steps of firstly, preparing the substance long-chain fatty alcohols (octacosanol) with low-surface-energy, and then octacosanol and polylactic acid exist
It is uniformly mixed in methylene chloride, realizes being blended for long-chain fatty alcohol and acid fiber by polylactic finally by electrostatic spinning.
The preparation method of a kind of super-hydrophobic acid fiber by polylactic of the present invention, which is characterized in that the method includes such as
Lower step:
(1) preparation of octacosanol: the rice bran wax (production of Haining De Bang Chemical Co., Ltd.) for weighing certain mass immerses 2
~5g/L sodium hydrate aqueous solution, the bath raio of rice bran wax quality (g) and sodium hydrate aqueous solution volume (mL) are 1 ︰ 20~30,
95~98 DEG C continuously stir reaction 10~15 hours, after reaction, 2~5g/L hydrochloric acid solution are added and neutralizes, makes the pH of solution
It is 6~7,2~5g/L calcium chloride solution is then added, uniform stirring generates precipitating, and filtering removes waste liquid, then filter cake is used
45~55 DEG C of hot water washings, vacuum drying.Then, extractant is made using acetone, solid-to-liquid ratio is 1 ︰ 15~20, is extracted through 6~8 times
It takes, extract liquor is collected, be evaporated under reduced pressure at 45~50 DEG C, is made long-chain fatty alcohol (octacosanol).
(2) preparation of spinning solution: polylactic acid selects l-lactic acid, buying in Hubei far at Sai Chuan Science and Technology Ltd.,
Its molecular weight is about 1.3 × 105~5.3 × 105.The pure and mild polylactic acid of long-chain fat of step (1) preparation is dissolved in dichloro simultaneously
In methane, wherein long-chain fatty alcohol and the mass ratio of polylactic acid are 1 ︰ 20~25, are stirred continuously in course of dissolution, when dissolution
Between be 30~60min, until the transparent stable liquid of solution matched, is configured to mass concentration as 20~40% solution.
(3) spinning of acid fiber by polylactic: carrying out electrostatic spinning for the spinning solution that step (2) prepares on electrostatic spinning machine,
Electrostatic spinning machine schematic device is as shown in Figure 1, spinning condition are as follows: 5~15KV of voltage, 3~4ml/h of jet velocity, jet length
From 90~120mm.
(4) washing of fiber: step (3) treated fiber being immersed in 70~80 DEG C of hot water, and the time is 2~3 small
When, 1 ︰ 10~20 of bath raio.
(5) fiber oils: by the oil bath solution of step (4) treated fiber immerses 3~4g/L, (model: WD weaves
Finish, the production of Wujiang north village, often used in village names chemical fibre finish factory), oil bath temperature is 80~85 DEG C, and the time is 3~4 hours, 1 ︰ 15 of bath raio
~20.
(6) drying of fiber: by step (5), treated that fiber obtains after drying and processing that super-hydrophobic polylactic acid is fine
Dimension.
The present invention has following distinguishing feature:
(1) acid fiber by polylactic prepared by the present invention does breaking strength between 6.0~6.5cN/dtex, and dry fracture is stretched
Long rate is between 25.5%~27.0%；Its wet breaking strength between 4.0~5.0cN/dtex, stretch by the wet fracture of fiber
Between 29.5%~30.5%, the strength property of the acid fiber by polylactic of main strength property and market purchasing connects long rate
Closely.Cellulose fibre prepared by the present invention is a kind of acid fiber by polylactic of qualification.
(2) surface of acid fiber by polylactic prepared by the present invention has low-surface energy substance octacosanol, is spun into poly-
Acid fiber fabric, water droplet polylactic acid fiber fabrics apparent contact angle range between 153 °~156 °, and water droplet is being adopted
The apparent contact angle of the polylactic acid fiber fabrics of purchase only has 38.8 °.Surpass it is thus regarded that acid fiber by polylactic prepared by the present invention has
Hydrophobicity.After 20 washings, the apparent contact angle range of polylactic acid fiber fabrics is distributed in 150 °~152 °, this is further
Show that acid fiber by polylactic prepared by the present invention still has super-hydrophobicity after repeatedly washing.
(3) present invention prepares super-hydrophobic acid fiber by polylactic by electrospinning process, finds and prepares with low-surface-energy
Substance long-chain fatty alcohol (octacosanol), whole simple production process are cheap, and production process environmental pollution is small, answer
With having a extensive future.
Detailed description of the invention
Fig. 1 electrostatic spinning machine schematic device (1. power supplys；2. receiving shaft；3. jet stream；4. syringe needle；5. bracket；6. leading
Pipe；7. polymer solution；8. syringe；9. propeller)
Specific embodiment
The present invention is described in detail in embodiment described below.
Embodiment 1
(1) it the preparation of octacosanol: weighs 300 grams of rice bran wax (production of Haining De Bang Chemical Co., Ltd.) and immerses 2g/L
Sodium hydrate aqueous solution, rice bran wax quality (g) and the bath raio of sodium hydrate aqueous solution volume (mL) are 1 ︰ 20, are continuously stirred at 95 DEG C
Reaction 10 hours is mixed, after reaction, 2g/L hydrochloric acid solution is added and neutralizes, makes the pH 6.5 of solution, 2g/L chlorination is then added
Calcium solution, uniform stirring generate precipitating, and filtering removes waste liquid, then filter cake is washed with 45 DEG C of hot water, are dried in vacuo.Then,
Extractant is made using acetone, solid-to-liquid ratio is 1 ︰ 15, extracts through 6 times, extract liquor is collected, be evaporated under reduced pressure at 45 DEG C, long-chain is made
Fatty alcohol (octacosanol).
(2) preparation of spinning solution: polylactic acid selects l-lactic acid, buying in Hubei far at Sai Chuan Science and Technology Ltd.,
Its molecular weight is about 1.3 × 105~5.3 × 105.The pure and mild polylactic acid of long-chain fat of step (1) preparation is dissolved in dichloro simultaneously
In methane, wherein long-chain fatty alcohol and the mass ratio of polylactic acid are 1 ︰ 20, are stirred continuously in course of dissolution, dissolution time is
30min, until the transparent stable liquid of solution matched, being configured to mass concentration is 20% PLA solution.
(3) spinning of acid fiber by polylactic: carrying out electrostatic spinning for the spinning solution that step (2) prepares on electrostatic spinning machine,
Electrostatic spinning machine schematic device is as shown in Figure 1, spinning condition are as follows: voltage 5KV, jet velocity 3ml/h, spray distance 90mm.
(4) washing of fiber: step (3) treated fiber being immersed in 70 DEG C of hot water, and the time is 2 hours, bath raio
1 ︰ 15.
(5) fiber oils: by the oil bath solution (model: WD textile oil of step (4) treated fiber immerses 3g/L
Agent, the production of Wujiang north village, often used in village names chemical fibre finish factory), oil bath temperature is 80 DEG C, and the time is 3 hours, 1 ︰ 15 of bath raio.
(6) drying of fiber: by step (5), treated that fiber obtains super-hydrophobic acid fiber by polylactic after drying and processing
a。
Embodiment 2
(1) it the preparation of octacosanol: weighs 300 grams of rice bran wax (production of Haining De Bang Chemical Co., Ltd.) and immerses 3g/L
Sodium hydrate aqueous solution, rice bran wax quality (g) and the bath raio of sodium hydrate aqueous solution volume (mL) are 1 ︰ 25, are continuously stirred at 96 DEG C
Reaction 12 hours is mixed, after reaction, 3g/L hydrochloric acid solution is added and neutralizes, makes the pH 6.5 of solution, 3g/L chlorination is then added
Calcium solution, uniform stirring generate precipitating, and filtering removes waste liquid, then filter cake is washed with 50 DEG C of hot water, are dried in vacuo.Then,
Extractant is made using acetone, solid-to-liquid ratio is 1 ︰ 18, extracts through 7 times, extract liquor is collected, be evaporated under reduced pressure at 46 DEG C, long-chain is made
Fatty alcohol (octacosanol).
(2) preparation of spinning solution: polylactic acid selects l-lactic acid, buying in Hubei far at Sai Chuan Science and Technology Ltd.,
Its molecular weight is about 1.3 × 105~5.3 × 105.The pure and mild polylactic acid of long-chain fat of step (1) preparation is dissolved in dichloro simultaneously
In methane, wherein long-chain fatty alcohol and the mass ratio of polylactic acid are 1 ︰ 22, are stirred continuously in course of dissolution, dissolution time is
40min, until the transparent stable liquid of solution matched, being configured to mass concentration is 25% PLA solution.
(3) spinning of acid fiber by polylactic: carrying out electrostatic spinning for the spinning solution that step (2) prepares on electrostatic spinning machine,
Electrostatic spinning machine schematic device is as shown in Figure 1, spinning condition are as follows: voltage 8KV, jet velocity 4ml/h, spray distance 100mm.
(4) washing of fiber: step (3) treated fiber being immersed in 75 DEG C of hot water, and the time is 2.5 hours, bath
Than 1 ︰ 15.
(5) fiber oils: by the oil bath solution (model: WD textile oil of step (4) treated fiber immerses 3.5g/L
Agent, the production of Wujiang north village, often used in village names chemical fibre finish factory), oil bath temperature is 82 DEG C, and the time is 3.5 hours, 1 ︰ 18 of bath raio.
(6) drying of fiber: by step (5), treated that fiber obtains super-hydrophobic acid fiber by polylactic after drying and processing
b。
Embodiment 3
(1) it the preparation of octacosanol: weighs 300 grams of rice bran wax (production of Haining De Bang Chemical Co., Ltd.) and immerses 4g/L
Sodium hydrate aqueous solution, rice bran wax quality (g) and the bath raio of sodium hydrate aqueous solution volume (mL) are 1 ︰ 28, are continuously stirred at 95 DEG C
Reaction 14 hours is mixed, after reaction, 4g/L hydrochloric acid solution is added and neutralizes, makes the pH 6.8 of solution, 4g/L chlorination is then added
Calcium solution, uniform stirring generate precipitating, and filtering removes waste liquid, then filter cake is washed with 50 DEG C of hot water, are dried in vacuo.Then,
Extractant is made using acetone, solid-to-liquid ratio is 1 ︰ 18, extracts through 7 times, extract liquor is collected, be evaporated under reduced pressure at 46 DEG C, long-chain is made
Fatty alcohol (octacosanol).
(2) preparation of spinning solution: polylactic acid selects l-lactic acid, buying in Hubei far at Sai Chuan Science and Technology Ltd.,
Its molecular weight is about 1.3 × 105~5.3 × 105.The pure and mild polylactic acid of long-chain fat of step (1) preparation is dissolved in dichloro simultaneously
In methane, wherein long-chain fatty alcohol and the mass ratio of polylactic acid are 1 ︰ 24, are stirred continuously in course of dissolution, dissolution time is
50min, until the transparent stable liquid of solution matched, being configured to mass concentration is 30% PLA solution.
(3) spinning of acid fiber by polylactic: carrying out electrostatic spinning for the spinning solution that step (2) prepares on electrostatic spinning machine,
Electrostatic spinning machine schematic device is as shown in Figure 1, spinning condition are as follows: voltage 8KV, jet velocity 3ml/h, spray distance 110mm.
(4) washing of fiber: step (3) treated fiber being immersed in 75 DEG C of hot water, and the time is 2.5 hours, bath
Than 1 ︰ 20.
(5) fiber oils: by the oil bath solution (model: WD textile oil of step (4) treated fiber immerses 3.5g/L
Agent, the production of Wujiang north village, often used in village names chemical fibre finish factory), oil bath temperature is 80 DEG C, and the time is 3 hours, 1 ︰ 15 of bath raio.
(6) drying of fiber: by step (5), treated that fiber obtains super-hydrophobic acid fiber by polylactic after drying and processing
c。
Embodiment 4
(1) it the preparation of octacosanol: weighs 300 grams of rice bran wax (production of Haining De Bang Chemical Co., Ltd.) and immerses 5g/L
Sodium hydrate aqueous solution, rice bran wax quality (g) and the bath raio of sodium hydrate aqueous solution volume (mL) are 1 ︰ 30, are continuously stirred at 98 DEG C
Reaction 15 hours is mixed, after reaction, 5g/L hydrochloric acid solution is added and neutralizes, makes the pH 7 of solution, 5g/L calcium chloride is then added
Solution, uniform stirring generate precipitating, and filtering removes waste liquid, then filter cake is washed with 55 DEG C of hot water, are dried in vacuo.Then, it adopts
Make extractant with acetone, solid-to-liquid ratio is 1 ︰ 20, extracts through 8 times, extract liquor is collected, be evaporated under reduced pressure at 50 DEG C, long-chain rouge is made
Fat alcohol (octacosanol).
(2) preparation of spinning solution: polylactic acid selects l-lactic acid, buying in Hubei far at Sai Chuan Science and Technology Ltd.,
Its molecular weight is about 1.3 × 105~5.3 × 105.The pure and mild polylactic acid of long-chain fat of step (1) preparation is dissolved in dichloro simultaneously
In methane, wherein long-chain fatty alcohol and the mass ratio of polylactic acid are 1 ︰ 25, are stirred continuously in course of dissolution, dissolution time is
60min, until the transparent stable liquid of solution matched, being configured to mass concentration is 40% PLA solution.
(3) spinning of acid fiber by polylactic: carrying out electrostatic spinning for the spinning solution that step (2) prepares on electrostatic spinning machine,
Electrostatic spinning machine schematic device is as shown in Figure 1, spinning condition are as follows: voltage 15KV, jet velocity 4ml/h, spray distance
120mm。
(4) washing of fiber: step (3) treated fiber being immersed in 80 DEG C of hot water, and the time is 3 hours, bath raio
1 ︰ 20.
(5) fiber oils: by the oil bath solution (model: WD textile oil of step (4) treated fiber immerses 4g/L
Agent, the production of Wujiang north village, often used in village names chemical fibre finish factory), oil bath temperature is 85 DEG C, and the time is 4 hours, 1 ︰ 20 of bath raio.
(6) drying of fiber: by step (5), treated that fiber obtains super-hydrophobic acid fiber by polylactic after drying and processing
d。
Embodiment 5
(1) it the preparation of octacosanol: weighs 300 grams of rice bran wax (production of Haining De Bang Chemical Co., Ltd.) and immerses 4g/L
Sodium hydrate aqueous solution, rice bran wax quality (g) and the bath raio of sodium hydrate aqueous solution volume (mL) are 1 ︰ 28, are continuously stirred at 96 DEG C
Reaction 14 hours is mixed, after reaction, 4g/L hydrochloric acid solution is added and neutralizes, makes the pH 6.5 of solution, 4g/L chlorination is then added
Calcium solution, uniform stirring generate precipitating, and filtering removes waste liquid, then filter cake is washed with 45 DEG C of hot water, are dried in vacuo.Then,
Extractant is made using acetone, solid-to-liquid ratio is 1 ︰ 18, extracts through 6 times, extract liquor is collected, be evaporated under reduced pressure at 50 DEG C, long-chain is made
Fatty alcohol (octacosanol).
(2) preparation of spinning solution: polylactic acid selects l-lactic acid, buying in Hubei far at Sai Chuan Science and Technology Ltd.,
Its molecular weight is about 1.3 × 105~5.3 × 105.The pure and mild polylactic acid of long-chain fat of step (1) preparation is dissolved in dichloro simultaneously
In methane, wherein long-chain fatty alcohol and the mass ratio of polylactic acid are 1 ︰ 22, are stirred continuously in course of dissolution, dissolution time is
60min, until the transparent stable liquid of solution matched, being configured to mass concentration is 35% PLA solution.
(3) spinning of acid fiber by polylactic: carrying out electrostatic spinning for the spinning solution that step (2) prepares on electrostatic spinning machine,
Electrostatic spinning machine schematic device is as shown in Figure 1, spinning condition are as follows: voltage 10KV, jet velocity 4ml/h, spray distance
120mm。
(4) washing of fiber: step (3) treated fiber being immersed in 75 DEG C of hot water, and the time is 2.5 hours, bath
Than 1 ︰ 15.
(5) fiber oils: by the oil bath solution (model: WD textile oil of step (4) treated fiber immerses 3.5g/L
Agent, the production of Wujiang north village, often used in village names chemical fibre finish factory), oil bath temperature is 85 DEG C, and the time is 3 hours, 1 ︰ 15 of bath raio.
(6) drying of fiber: by step (5), treated that fiber obtains super-hydrophobic acid fiber by polylactic after drying and processing
e。
Performance evaluation example:
Super-hydrophobic acid fiber by polylactic a, b, c, d, e that specific embodiment 1~5 above-mentioned in the present invention is prepared are carried out strong
Power performance test, test method is with reference to GB/T-24218.3-2010 " textile, non-woven cloth test method third portion: fracture
The measurement of strength and elongation at break ", using the strong of the full-automatic single fiber universl tester measurement sample of FAVIMAT-BOBOT2
Power performance, test sample are no less than 30, take testing mean.Test result is as shown in table 1, wherein super-hydrophobic polylactic acid is fine
A, b, c, d, e abbreviation fiber a, b, c, d, e are tieed up, the acid fiber by polylactic of buying is from Haining Xin Neng Textile Co., Ltd..
The mechanical property of table 1 acid fiber by polylactic a, b, c, d, e and the acid fiber by polylactic bought by oneself
As seen from Table 1, the acid fiber by polylactic of preparation does breaking strength between 6.0~6.5cN/dtex, slightly below adopts
The acid fiber by polylactic of purchase, the dry elongation at break of the acid fiber by polylactic of preparation are slightly below purchased between 25.5%~27.0%
Acid fiber by polylactic；For the acid fiber by polylactic wet breaking strength of preparation between 4.0~5.0cN/dtex, that slightly below purchases is poly-
Acid fiber, the wet elongation at break of the acid fiber by polylactic of preparation is between 29.5%~30.5%, the poly- cream slightly below purchased
Sour fiber.From the point of view of the test result of mechanical property, the main mechanical properties of acid fiber by polylactic prepared by the present invention and Haining are new
The acid fiber by polylactic of energy Textile Co., Ltd. is relatively, it can be seen that, cellulose fibre prepared by the present invention is a kind of qualification
Acid fiber by polylactic.
It, will be above-mentioned in the present invention in order to preferably detect the super-hydrophobicity of the super-hydrophobic acid fiber by polylactic prepared in the present invention
The acid fiber by polylactic of super-hydrophobic acid fiber by polylactic a, b, c, d, e and buying that specific embodiment 1~5 is prepared are using identical
Technique, the acid fiber by polylactic for being spun into polylactic acid fiber fabrics a, b, c, d, e (abbreviation fabric a, b, c, d, e) and buying are knitted
Object.Apparent contact angle using XG-CAMA1 basic model contact angle tester measurement water droplet on polylactic acid fiber fabrics surface, is surveyed
Sample of having a try is no less than 30, takes testing mean, and test result is as shown in table 2.
Apparent contact angle of 2 water droplet of table in polylactic acid fiber fabrics a, b, c, d, e and the polylactic acid fiber fabrics bought by oneself
As seen from Table 2, water droplet the apparent contact angle range of polylactic acid fiber fabrics a, b, c, d, e be distributed in 153 °~
Between 156 °, and the apparent contact angle for the polylactic acid fiber fabrics purchased only has 38.8 °.Under normal conditions, work as apparent contact angle
When greater than 150 °, illustrate that the fabric has super-hydrophobicity.It is possible thereby to think, acid fiber by polylactic prepared by the present invention has super thin
It is aqueous.
In order to preferably detect being influenced by washing for the acid fiber by polylactic ultra-hydrophobicity prepared in the present invention, reference
GB/T 20944.1-2007 color fastness to washing testing machine washing methods carries out standard to polylactic acid fiber fabrics a, b, c, d, e and washes
It washs, after passing it through 20 washings, tests its ultra-hydrophobicity, test result such as table 3 again.
Apparent contact of 3 water droplet of table in polylactic acid fiber fabrics and the polylactic acid fiber fabrics of buying after 20 washings
Angle
As seen from Table 3, after 20 washings, the apparent contact angle range of polylactic acid fiber fabrics a, b, c, d, e are distributed
Between 150 °~152 °, and the apparent contact angle for the polylactic acid fiber fabrics purchased only has 35.7 °.It is possible thereby to think, this
The acid fiber by polylactic for inventing preparation still has super-hydrophobicity after repeatedly washing.
Claims (8)
1. a kind of preparation method of super-hydrophobic acid fiber by polylactic, which is characterized in that described method includes following steps:
(1) preparation of octacosanol: weigh certain mass rice bran wax (production of Haining De Bang Chemical Co., Ltd.) immerse 2~
5g/L sodium hydrate aqueous solution continuously stirs reaction 10~15 hours at 95~98 DEG C, after reaction, 2~5g/L salt is added
Acid solution neutralizes, and makes the pH 6~7 of solution, and 2~5g/L calcium chloride solution is then added, and uniform stirring generates precipitating, mistake
Filter removes waste liquid, then filter cake is washed with 45~55 DEG C of hot water, is dried in vacuo.Then, extractant is made using organic solvent, Gu
Liquor ratio is 1 ︰ 15~20, extracts through 6~8 times, extract liquor is collected, and is evaporated under reduced pressure at 45~50 DEG C, and long-chain fatty alcohol (two is made
Octadecyl alcolol).
(2) preparation of spinning solution: polylactic acid selects l-lactic acid, buying in Hubei far at Sai Chuan Science and Technology Ltd., point
Son amount about 1.3 × 105~5.3 × 105.The pure and mild polylactic acid of long-chain fat of step (1) preparation is dissolved in methylene chloride simultaneously
In, it being stirred continuously in course of dissolution, dissolution time is 30~60min, until the transparent stable liquid of solution matched,
It is configured to the solution of certain mass concentration.
(3) spinning solution that step (2) prepares the spinning of acid fiber by polylactic: is subjected to electrostatic spinning, electrostatic on electrostatic spinning machine
Spinning machine schematic device is as shown in Figure 1, spinning condition are as follows: suitable voltage, jet velocity and spray distance.
(4) washing of fiber: step (3) treated fiber being immersed in the hot water of certain temperature, and the time is 2~3 hours, bath
Than 1 ︰ 10~20.
(5) fiber oils: by step (4), treated that fiber immerses certain density oil bath solution (model: WD textile oil
Agent, the production of Wujiang north village, often used in village names chemical fibre finish factory), oil bath temperature is 80~85 DEG C, and the time is 3~4 hours, 1 ︰ 15 of bath raio~
20。
(6) drying of fiber: by step (5), treated that fiber obtains super-hydrophobic acid fiber by polylactic after drying and processing.
2. the preparation method of a kind of super-hydrophobic acid fiber by polylactic according to claim 1, it is characterized in that the step (1)
The bath raio of middle rice bran wax quality (g) and sodium hydrate aqueous solution volume (mL) are 1 ︰ 20~30.
3. the preparation method of a kind of super-hydrophobic acid fiber by polylactic according to claim 1, it is characterized in that the step (1)
Middle extractant is acetone.
4. the preparation method of a kind of super-hydrophobic acid fiber by polylactic according to claim 1, it is characterized in that the step (2)
The middle long-chain fatty alcohol dissolved in methylene chloride and the mass ratio of polylactic acid are 1 ︰ 20~25.
5. the preparation method of a kind of super-hydrophobic acid fiber by polylactic according to claim 1, it is characterized in that the step (2)
In be configured to solution mass concentration be 20~40%.
6. the preparation method of a kind of super-hydrophobic acid fiber by polylactic according to claim 1, it is characterized in that the step (3)
Middle spinning condition are as follows: voltage is 5~15KV, and jet velocity is 3~4ml/h, and spray distance is 90~120mm.
7. the preparation method of a kind of super-hydrophobic acid fiber by polylactic according to claim 1, it is characterized in that the step (4)
The temperature of middle hot water is 70~80 DEG C.
8. the preparation method of a kind of super-hydrophobic acid fiber by polylactic according to claim 1, it is characterized in that the step (5)
The concentration of middle oil bath solution is 3~4g/L.
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